#------------------------------------------------------------------------------
#$Date: 2016-02-25 08:56:43 +0200 (Thu, 25 Feb 2016) $
#$Revision: 176918 $
#$URL: svn://www.crystallography.net/cod/cif/7/10/38/7103865.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_7103865
loop_
_publ_author_name
'Chen, Banglin'
'Fronczek, Frank R'
'Maverick, Andrew W'
_publ_section_title
;
 Solvent-dependent 4(4) square grid and 6(4).8(2) NbO frameworks formed
 by Cu(Pyac)2 (bis[3-(4-pyridyl)pentane-2,4-dionato]copper(II)).
;
_journal_issue                   17
_journal_name_full
'Chemical communications (Cambridge, England)'
_journal_page_first              2166
_journal_page_last               2167
_journal_paper_doi               10.1039/b305457h
_journal_year                    2003
_chemical_compound_source        'local laboratory'
_chemical_formula_moiety         'C22 H30 Cu N2 O7'
_chemical_formula_sum            'C22 H30 Cu N2 O7'
_chemical_formula_weight         498.02
_chemical_name_common
;Bis(3-(4-pyridyl)-2,4-pentanedionato)copper(ii), ethanol-
water solvate
;
_chemical_name_systematic
;
Bis(3-(4-pyridyl)-2,4-pentanedionato)copper(II), ethanol-water solvate
;
_space_group_IT_number           167
_symmetry_cell_setting           trigonal
_symmetry_space_group_name_Hall  '-R 3 2"c'
_symmetry_space_group_name_H-M   'R -3 c :H'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            18
_cell_length_a                   22.604(2)
_cell_length_b                   22.604(2)
_cell_length_c                   22.964(3)
_cell_measurement_reflns_used    8847
_cell_measurement_temperature    100
_cell_measurement_theta_max      33.7
_cell_measurement_theta_min      2.5
_cell_volume                     10161.3(18)
_computing_cell_refinement
'Denzo and Scalepack (Otwinowski & Minor, 1997)'
_computing_data_collection       'COLLECT (Nonius 1999)'
_computing_data_reduction
'Denzo and Scalepack (Otwinowski & Minor, 1997)'
_computing_molecular_graphics    'ORTEP-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution
'Direct_methods (SIR, Altomare, et al., 1994)'
_diffrn_ambient_temperature      100
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device       'KappaCCD (with Oxford Cryostream)'
_diffrn_measurement_method       ' ω scans with κ offsets'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.028
_diffrn_reflns_av_sigmaI/netI    0.0245
_diffrn_reflns_limit_h_max       35
_diffrn_reflns_limit_h_min       -35
_diffrn_reflns_limit_k_max       30
_diffrn_reflns_limit_k_min       -30
_diffrn_reflns_limit_l_max       35
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            45659
_diffrn_reflns_theta_full        33.7
_diffrn_reflns_theta_max         33.7
_diffrn_reflns_theta_min         2.7
_diffrn_standards_decay_%        <2
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.013
_exptl_absorpt_correction_T_max  0.761
_exptl_absorpt_correction_T_min  0.706
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'HKL Scalepack (Otwinowski & Minor 1997)'
_exptl_crystal_colour            'greenish blue'
_exptl_crystal_density_diffrn    1.465
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             4698
_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.47
_exptl_crystal_size_min          0.27
_refine_diff_density_max         0.90
_refine_diff_density_min         -1.05
_refine_diff_density_rms         0.101
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.459
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     168
_refine_ls_number_reflns         4517
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.459
_refine_ls_R_factor_all          0.054
_refine_ls_R_factor_gt           0.043
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0699P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.136
_refine_ls_wR_factor_ref         0.143
_reflns_number_gt                3687
_reflns_number_total             4517
_reflns_threshold_expression     I>2σ(I)
_cod_data_source_file            b305457h.txt
_cod_data_source_block           BChen_compound_1
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Trigonal' changed to 'trigonal' according
to '/home/saulius/struct/CIF-dictionaries/cif_core.dic' dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 
;
_cod_original_sg_symbol_H-M      'R -3 c        '
_cod_original_formula_sum        'C20 H20 Cu N2 O4, C2 H6 O, 2(H2O)'
_cod_database_code               7103865
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'x-y, -y, -z+1/2'
'-x, -x+y, -z+1/2'
'y, x, -z+1/2'
'x+2/3, y+1/3, z+1/3'
'-y+2/3, x-y+1/3, z+1/3'
'-x+y+2/3, -x+1/3, z+1/3'
'x-y+2/3, -y+1/3, -z+5/6'
'-x+2/3, -x+y+1/3, -z+5/6'
'y+2/3, x+1/3, -z+5/6'
'x+1/3, y+2/3, z+2/3'
'-y+1/3, x-y+2/3, z+2/3'
'-x+y+1/3, -x+2/3, z+2/3'
'x-y+1/3, -y+2/3, -z+7/6'
'-x+1/3, -x+y+2/3, -z+7/6'
'y+1/3, x+2/3, -z+7/6'
'-x, -y, -z'
'y, -x+y, -z'
'x-y, x, -z'
'-x+y, y, z-1/2'
'x, x-y, z-1/2'
'-y, -x, z-1/2'
'-x+2/3, -y+1/3, -z+1/3'
'y+2/3, -x+y+1/3, -z+1/3'
'x-y+2/3, x+1/3, -z+1/3'
'-x+y+2/3, y+1/3, z-1/6'
'x+2/3, x-y+1/3, z-1/6'
'-y+2/3, -x+1/3, z-1/6'
'-x+1/3, -y+2/3, -z+2/3'
'y+1/3, -x+y+2/3, -z+2/3'
'x-y+1/3, x+2/3, -z+2/3'
'-x+y+1/3, y+2/3, z+1/6'
'x+1/3, x-y+2/3, z+1/6'
'-y+1/3, -x+2/3, z+1/6'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Cu1 Cu 0.0000 0.5000 0.0000 0.01560(9) Uani 1 2 d S . .
O1 O 0.07941(5) 0.48902(5) 0.00893(4) 0.01840(19) Uani 1 1 d . . .
O2 O -0.04539(5) 0.43910(5) 0.06441(4) 0.01824(19) Uani 1 1 d . . .
N1 N 0.13073(6) 0.38571(6) 0.25417(5) 0.0188(2) Uani 1 1 d . . .
C1 C 0.16661(7) 0.47882(9) 0.05496(7) 0.0262(3) Uani 1 1 d . . .
H1A H 0.1818 0.4817 0.0146 0.039 Uiso 1 1 calc R . .
H1B H 0.1651 0.4393 0.0740 0.039 Uiso 1 1 calc R . .
H1C H 0.1986 0.5206 0.0758 0.039 Uiso 1 1 calc R . .
C2 C 0.09630(7) 0.47098(6) 0.05573(6) 0.0175(2) Uani 1 1 d . . .
C3 C 0.05387(6) 0.44328(6) 0.10517(6) 0.0168(2) Uani 1 1 d . . .
C4 C -0.01485(7) 0.42842(6) 0.10625(5) 0.0168(2) Uani 1 1 d . . .
C5 C -0.05875(8) 0.39673(8) 0.15937(6) 0.0222(3) Uani 1 1 d . . .
H5A H -0.0952 0.4082 0.1603 0.033 Uiso 1 1 calc R . .
H5B H -0.0306 0.4145 0.1945 0.033 Uiso 1 1 calc R . .
H5C H -0.0789 0.3470 0.1578 0.033 Uiso 1 1 calc R . .
C6 C 0.08114(7) 0.42426(7) 0.15685(6) 0.0176(2) Uani 1 1 d . . .
C7 C 0.05480(7) 0.35604(7) 0.17235(6) 0.0217(3) Uani 1 1 d . . .
H7 H 0.0192 0.3210 0.1499 0.026 Uiso 1 1 calc R . .
C8 C 0.08047(7) 0.33917(7) 0.22054(6) 0.0216(3) Uani 1 1 d . . .
H8 H 0.0615 0.2923 0.2302 0.026 Uiso 1 1 calc R . .
C9 C 0.15654(7) 0.45141(7) 0.23910(6) 0.0195(2) Uani 1 1 d . . .
H9 H 0.1925 0.4852 0.2621 0.023 Uiso 1 1 calc R . .
C10 C 0.13362(7) 0.47285(7) 0.19170(6) 0.0198(2) Uani 1 1 d . . .
H10 H 0.1535 0.5201 0.1831 0.024 Uiso 1 1 calc R . .
O1S O 0.1919(3) 0.5747(3) -0.0746(3) 0.0856(16) Uani 0.50 1 d P A 1
C1S C 0.2067(4) 0.6117(4) -0.0256(4) 0.079(2) Uani 0.50 1 d P A 1
C2S C 0.2516(4) 0.6737(4) 0.0016(4) 0.085(2) Uani 0.50 1 d P A 1
O2S O 0.1919(2) 0.6128(2) -0.0650(3) 0.0709(13) Uani 0.50 1 d P B 2
O3S O 0.2933(4) 0.6785(4) 0.0178(3) 0.0679(16) Uiso 0.33 1 d P C 2
O4S O 0.0000 0.0000 0.0000 0.235(8) Uani 1 6 d S . .
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O2 Cu1 O2 180.0 19_565 . ?
O2 Cu1 O1 88.65(4) 19_565 . ?
O2 Cu1 O1 91.35(4) . . ?
O2 Cu1 O1 91.35(4) 19_565 19_565 ?
O2 Cu1 O1 88.65(4) . 19_565 ?
O1 Cu1 O1 180.0 . 19_565 ?
O2 Cu1 N1 96.68(4) 19_565 26_455 ?
O2 Cu1 N1 83.32(4) . 26_455 ?
O1 Cu1 N1 85.80(4) . 26_455 ?
O1 Cu1 N1 94.20(4) 19_565 26_455 ?
O2 Cu1 N1 83.32(4) 19_565 14_554 ?
O2 Cu1 N1 96.68(4) . 14_554 ?
O1 Cu1 N1 94.20(4) . 14_554 ?
O1 Cu1 N1 85.80(4) 19_565 14_554 ?
N1 Cu1 N1 180 26_455 14_554 ?
C2 O1 Cu1 125.04(9) . . ?
C4 O2 Cu1 124.60(9) . . ?
C8 N1 Cu1 113.15(9) . 9_455 ?
C9 N1 Cu1 130.05(9) . 9_455 ?
C8 N1 C9 116.67(11) . . ?
C2 C1 H1A 109.5 . . ?
C2 C1 H1B 109.5 . . ?
H1A C1 H1B 109.5 . . ?
C2 C1 H1C 109.5 . . ?
H1A C1 H1C 109.5 . . ?
H1B C1 H1C 109.5 . . ?
O1 C2 C3 124.99(12) . . ?
O1 C2 C1 114.78(12) . . ?
C3 C2 C1 120.19(12) . . ?
C2 C3 C4 122.67(12) . . ?
C2 C3 C6 118.57(12) . . ?
C4 C3 C6 118.61(12) . . ?
O2 C4 C3 125.15(12) . . ?
O2 C4 C5 114.18(12) . . ?
C3 C4 C5 120.67(11) . . ?
C4 C5 H5A 109.5 . . ?
C4 C5 H5B 109.5 . . ?
H5A C5 H5B 109.5 . . ?
C4 C5 H5C 109.5 . . ?
H5A C5 H5C 109.5 . . ?
H5B C5 H5C 109.5 . . ?
C7 C6 C10 116.66(13) . . ?
C7 C6 C3 120.76(12) . . ?
C10 C6 C3 122.58(12) . . ?
C8 C7 C6 120.11(13) . . ?
C8 C7 H7 119.9 . . ?
C6 C7 H7 119.9 . . ?
N1 C8 C7 123.36(13) . . ?
N1 C8 H8 118.3 . . ?
C7 C8 H8 118.3 . . ?
N1 C9 C10 123.74(12) . . ?
N1 C9 H9 118.1 . . ?
C10 C9 H9 118.1 . . ?
C9 C10 C6 119.45(12) . . ?
C9 C10 H10 120.3 . . ?
C6 C10 H10 120.3 . . ?
O1S C1S C2S 145.9(7) . . ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Cu1 O2 1.9295(10) 19_565 ?
Cu1 O2 1.9296(9) . ?
Cu1 O1 1.9419(10) . ?
Cu1 O1 1.9420(10) 19_565 ?
Cu1 N1 2.5156(12) 26_455 ?
Cu1 N1 2.5156(12) 14_554 ?
O1 C2 1.2739(15) . ?
O2 C4 1.2746(15) . ?
N1 C8 1.3411(18) . ?
N1 C9 1.3414(18) . ?
C1 C2 1.5087(19) . ?
C1 H1A 0.9800 . ?
C1 H1B 0.9800 . ?
C1 H1C 0.9800 . ?
C2 C3 1.4144(19) . ?
C3 C4 1.4158(19) . ?
C3 C6 1.496(2) . ?
C4 C5 1.5083(19) . ?
C5 H5A 0.9800 . ?
C5 H5B 0.9800 . ?
C5 H5C 0.9800 . ?
C6 C7 1.3932(19) . ?
C6 C10 1.3969(18) . ?
C7 C8 1.3884(18) . ?
C7 H7 0.9500 . ?
C8 H8 0.9500 . ?
C9 C10 1.3925(18) . ?
C9 H9 0.9500 . ?
C10 H10 0.9500 . ?
O1S C1S 1.342(11) . ?
C1S C2S 1.400(11) . ?
_cod_duplicate_entry 7113851
